WO2003051962A1 - Procede de production de sels d'acides humiques - Google Patents

Procede de production de sels d'acides humiques Download PDF

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Publication number
WO2003051962A1
WO2003051962A1 PCT/RU2002/000533 RU0200533W WO03051962A1 WO 2003051962 A1 WO2003051962 A1 WO 2003051962A1 RU 0200533 W RU0200533 W RU 0200533W WO 03051962 A1 WO03051962 A1 WO 03051962A1
Authority
WO
WIPO (PCT)
Prior art keywords
oxidation
lignin
product
mixture
stage
Prior art date
Application number
PCT/RU2002/000533
Other languages
English (en)
Russian (ru)
Inventor
Oleg Andreevich Gladkov
Rodion Borisovich Poloskin
Yury Jurievich Polyakov
Irina Vasilievna Sokolova
Nikolay Ivanovich Sorokin
Aleksey Valerievich Glebov
Original Assignee
Obschestvo S Ogranichennoy Otvetsvennostyu 'nauchno Proizvostvennoe Obiedinenie 'realizatsia Ekologicheskih Tehnology'
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Obschestvo S Ogranichennoy Otvetsvennostyu 'nauchno Proizvostvennoe Obiedinenie 'realizatsia Ekologicheskih Tehnology' filed Critical Obschestvo S Ogranichennoy Otvetsvennostyu 'nauchno Proizvostvennoe Obiedinenie 'realizatsia Ekologicheskih Tehnology'
Priority to US10/498,776 priority Critical patent/US7198805B2/en
Priority to EA200400725A priority patent/EA006824B1/ru
Priority to AU2002362155A priority patent/AU2002362155A1/en
Priority to UA20040705797A priority patent/UA76563C2/uk
Publication of WO2003051962A1 publication Critical patent/WO2003051962A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H99/00—Subject matter not provided for in other groups of this subclass, e.g. flours, kernels

Definitions

  • PROCESSING PRODUCTS ARE SUBJECT TO MATERIALS RELATED TO COMPONENT COMPOSITION AND PHYSICAL PROPERTIES TO HUMAL SALES. These products can be used in agriculture as a stimulating fertilizer, in the form of agronomic fertilizers, and as an agglomerate
  • the method was known ( ⁇ its ⁇ . ⁇ ., Shchuplyak ⁇ . ⁇ ., Gladkov ⁇ . ⁇ ., Sokolova I. ⁇ ., Pelevin L. ⁇ . s ⁇ chny ⁇ v ⁇ d, ⁇ y ⁇ bes ⁇ echivae ⁇ ⁇ b ⁇ az ⁇ vanie guma ⁇ v ⁇ u ⁇ em mixing s ⁇ chny ⁇ v ⁇ d with schel ⁇ chnym agen ⁇ m, a ⁇ ivatsii ⁇ ea ⁇ tsi ⁇ nn ⁇ y mixture gid ⁇ dinamiches ⁇ im ⁇ avi ⁇ atsi ⁇ nnym v ⁇ zdeys ⁇ viem ⁇ i ⁇ em ⁇ e ⁇ a ⁇ u ⁇ e 50- 170 ° C ⁇ dn ⁇ v ⁇ emenn ⁇ y ⁇ dachey szha ⁇ g ⁇ v ⁇ zdu ⁇ a ⁇ d pressure 0,2-1, 6 ⁇ Pa.
  • the prepared mixture is heated to a working temperature of 140-190 ° C and is charged to a process with a compressed air, it is consumed by the S ⁇ s ⁇ b ⁇ lucheniya gumin ⁇ v ⁇ g ⁇ ⁇ ntsen ⁇ a ⁇ a of ⁇ i ⁇ dny ⁇ gumi ⁇ v and ⁇ aus ⁇ bi ⁇ li ⁇ v ug ⁇ ln ⁇ g ⁇ ⁇ yada s ⁇ glasn ⁇ iz ⁇ b ⁇ e ⁇ eniyu s ⁇ de ⁇ zhi ⁇ gid ⁇ a ⁇ i ⁇ vannye gumin ⁇ vye ⁇ isl ⁇ y, s ⁇ li gumin ⁇ vy ⁇ ⁇ isl ⁇ and mine ⁇ alnye ⁇ m ⁇ nen ⁇ y is ⁇ dny ⁇ gumi ⁇ v and ⁇ aus ⁇ bi ⁇ li ⁇ v, ⁇ imiches ⁇ i related s ⁇ de ⁇ zhaschimisya gumin ⁇ vymi ⁇ isl ⁇ ami.
  • the invention is aimed at the emission of salt of humic acid in a continuous mode and with a high yield of useful products.
  • the problem is solved in that the process of liquid-liquid oxidation of a mixture of an alkaline agent with a lignite-containing plant material, with a total dry matter content of 12-20%, is free from moisture.
  • Pe ⁇ vaya s ⁇ adiya ⁇ ed ⁇ isleniya ⁇ v ⁇ di ⁇ sya ⁇ i ⁇ em ⁇ e ⁇ a ⁇ u ⁇ e 50-190 ° C and pressures from 0.5-3 ⁇ Pa ⁇ dn ⁇ v ⁇ emenn ⁇ y ⁇ b ⁇ ab ⁇ y ⁇ isl ⁇ d ⁇ s ⁇ de ⁇ z haschim gaz ⁇ m d ⁇ d ⁇ s ⁇ izheniya ⁇ 10,5-12, and v ⁇ aya - ⁇ islenie in ⁇ e ⁇ same usl ⁇ viya ⁇ ⁇ i ⁇ em ⁇ e ⁇ a ⁇ u ⁇ e 170-210 ° C, pressure 0.5-3 ⁇ As far as reaching ⁇ 8.5-10.
  • oxidation can result in oxygen-containing gases with a specific gas flow rate of 20-65 nm 3 / m 3 h.
  • the circulating material is used for additional activation of the mixture of lignin-containing vegetative raw materials with alkali in the cavitating mode.
  • the first stage may be through oxidation of the inoculum, and also not in the process of the use of the product through the use of a
  • a waste product mixture to a mixture of a lignite-containing raw material with an alkali at a temperature below 50 ° C is inappropriate and does not allow the product to be removed. For example, for example, temperature and temperature of 20 ° C, it takes 5-6 hours to recover the food.
  • the output should be at least 12, since the input of the external process is only 12%, the percentage of the input is 12%.
  • the development of chinones which are simply a place for further compensation of high-molecular humic substances, is noted only for more than 12.
  • Acidification of lignite-containing raw materials which are distinguished by the fact that it is disposed of by acid, which is acid-hazardous Due to the mechanical mechanism and the partial disintegration of the product, it is necessary to increase the consumption of strongly disproportionate components to the product.
  • An increase in processing time of more than 60 minutes does not “ not ” result in an increase in the content of chronic and acid groups.
  • the original lignosulfonates in the amount of 100 kg dilute 250 liters of water and mix with 12 kg (30% of the total mass of organic matter) diluted with 50 liters of water.
  • the mixture is heated in a heat exchanger to a temperature of 180 ° C and with a pump that passes through a heat exchanger, it is loaded into a process-converter, after which it is heated There is a blasting of air with a pressure of 2.0 PSa with a specific flow rate of up to 20-30nm 3 / m 3 .
  • the lignosulfonate mixture is heated with heat in a heat exchanger up to 70 ° C and poured into a separate reaction. Whereas, over a period of 0.5 hours, 28.7 liters are poured (6% of the content of household substances), a couple of 12% of the water consumed are consumed.
  • the cassette is heated to 85 ° C, the mass is left for 45 minutes, and at a low temperature it drops to 70 ° C.
  • the lignus processing unit is used as shown in Example 2. After reaching ⁇ 10, the mass is empty, where it is cooled, it is supplied for 100 ° C. However, the resultant dry salts are saturated with trace elements and acid in the following quantities: ⁇ 4 -5 ⁇ 2 ⁇ - 351, 0 g containing 80 g ⁇
  • the lignosulfonate mixture is heated with heat in a heat exchanger up to 50 ° C and poured into a separate reaction. Whereas, over a period of 0.5 hours, 28.7 liters are poured (6% of the content of household substances), a couple of 12% of the water consumed are consumed. The pan is heated to 85 ° C, the mass is left at 45 minutes, and at a low temperature it is reduced to 70 ° C.
  • the original lignosulfones of example 1 in the amount of 100 kg are diluted with 250 liters of water and mixed with 12 kg (30% of the mass of industrial water), 50 ml.
  • the mixture is heated in a heat exchanger to a temperature of 190 ° C and with a pump that passes through a heat exchanger, it is loaded into a process-converter, after which it is heated There is a blasting of air with a pressure of 2.0 PSa with a specific flow rate of up to 20 nm 3 / m 3
  • lignin was used - a convenient product of hydraulic product.
  • Table 1 shows the finished products depending on the conditions of oxidation, which helps to ensure that the product is in good condition.
  • ⁇ ⁇ tsesse ⁇ ed ⁇ isleniya ⁇ isl ⁇ d ⁇ m v ⁇ zdu ⁇ a or ⁇ e ⁇ e ⁇ isyu v ⁇ d ⁇ da ⁇ d influence ⁇ em ⁇ e ⁇ a ⁇ u ⁇ y 50-190 ° C sul ⁇ g ⁇ u ⁇ y gid ⁇ lizuyu ⁇ sya and ⁇ b ⁇ azuyuschiesya ⁇ i e ⁇ m ⁇ en ⁇ ly ⁇ bladayu ⁇ vys ⁇ y ⁇ ea ⁇ tsi ⁇ nn ⁇ y s ⁇ s ⁇ bn ⁇ s ⁇ yu ⁇ ⁇ ea ⁇ tsiyam ⁇ e ⁇ eg ⁇ u ⁇ i ⁇ v ⁇ i with ⁇ sche ⁇ leniem b ⁇ vy ⁇ tse ⁇ ey and ⁇ li ⁇ ndensatsiey.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Fertilizers (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

Selon cette invention, des sels d'acides humiques à haut pourcentage de produits utiles sont obtenus par oxydation en phase liquide d'un mélange composé d'un agent alcalin et d'une matière première végétale à base de lignine présentant une teneur en substances sèches comprise entre 12 et 20 %, laquelle oxydation est effectuée selon un procédé continu en deux étapes. Dans la première étape, une pré-oxydation est effectuée à une température comprise entre 50 et 190 °C et à une pression comprise entre 0,5 et 3 MPa, laquelle pré-oxydation est effectuée simultanément à un traitement au gaz à base d'oxygène jusqu'à ce qu'on obtienne un pH compris entre 10,5 et 12. Dans la seconde étape, l'oxydation est effectuée dans les mêmes conditions que dans la première étape, mais à une température comprise entre 170 et 200 °C jusqu'à ce qu'on obtienne un pH compris entre 8,5 et 10. Un sous-produit émanant de la production de cellulose par un procédé au sulfite, à savoir des solutions concentrées de lignosulfonate ou de lignine, laquelle lignine est un sous-produit de la production par hydrolyse, est utilisé comme matière première végétale à base de lignine, et est oxydé par l'oxygène de l'air dans un procédé continu en deux étapes. Afin d'activer davantage le mélange composé de matière première et d'agent alcalin dans un mode de cavitation, on peut utiliser une pompe de circulation équipée d'un éjecteur assurant l'expulsion de l'air. Afin de réduire le temps de pré-oxydation, la première étape peut être mise en oeuvre à l'aide de peroxyde d'hydrogène ou au moyen de matière première et d'agent alcalin introduits directement dans une conduite située en amont de l'éjecteur avant le mélange avec l'agent oxydant.
PCT/RU2002/000533 2001-12-19 2002-12-16 Procede de production de sels d'acides humiques WO2003051962A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US10/498,776 US7198805B2 (en) 2001-12-19 2002-12-16 Method for producing humic acid salts
EA200400725A EA006824B1 (ru) 2001-12-19 2002-12-16 Способ получения солей гуминовых кислот
AU2002362155A AU2002362155A1 (en) 2001-12-19 2002-12-16 Method for producing humic acid salts
UA20040705797A UA76563C2 (en) 2001-12-19 2002-12-16 Method for producing humic acids salts

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2001134139/04A RU2205166C1 (ru) 2001-12-19 2001-12-19 Способ получения солей гуминовых кислот
RU2001134139 2001-12-19

Publications (1)

Publication Number Publication Date
WO2003051962A1 true WO2003051962A1 (fr) 2003-06-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/RU2002/000533 WO2003051962A1 (fr) 2001-12-19 2002-12-16 Procede de production de sels d'acides humiques

Country Status (6)

Country Link
US (1) US7198805B2 (fr)
AU (1) AU2002362155A1 (fr)
EA (1) EA006824B1 (fr)
RU (1) RU2205166C1 (fr)
UA (1) UA76563C2 (fr)
WO (1) WO2003051962A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
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CN115364640A (zh) * 2022-08-03 2022-11-22 广西壮族自治区海洋环境监测中心站 一种改性腐殖酸盐及其在强化氢氧化钙脱硫中的应用

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US20030044382A1 (en) * 2001-05-11 2003-03-06 Selvig Thomas A. Biologic-chemical herbicide compositions and methods of use
CA2668394A1 (fr) * 2006-11-03 2008-05-08 Bijam Biosciences Private Limited Fabrication de molecules organiques fonctionnellement efficaces provenant du clivage de la lignite
EP2099725A2 (fr) * 2006-11-15 2009-09-16 Bijam Biosciences Private Limited Lignite structuralement modifiée avec ou sans extraction de molécules organiques fonctionnellement améliorées
US20100303927A1 (en) * 2009-05-27 2010-12-02 Michael P Pompeo Composition and method for incorporating colorant into wood
UA116535C2 (uk) * 2012-03-30 2018-04-10 Рдінновейшн Апс Сполуки бензолполікарбонових кислот та їх застосування як лікарських засобів
WO2014193337A1 (fr) 2013-05-28 2014-12-04 Empire Technology Development Llc Dérivés d'acide humique antioxydants et procédés de préparation et d'utilisation
WO2014193338A1 (fr) 2013-05-28 2014-12-04 Empire Technology Development Llc Dérivés d'acide humique et procédés de préparation et d'utilisation
US10106570B2 (en) 2013-06-28 2018-10-23 Empire Technology Development Llc Edible plasticizers for food and food packaging films
US10233132B2 (en) * 2015-10-19 2019-03-19 Oleksandr Galaka Organic or organo-mineral fertilizers, method of producing thereof and production unit therefor
US10077216B2 (en) 2017-02-22 2018-09-18 Pro Farm Technologies Oy Soluble fertilizer formulation and method for use thereof
US11130903B2 (en) * 2017-05-09 2021-09-28 Halliburton Energy Services, Inc. Fulvic acid well treatment fluid
RU2738153C1 (ru) * 2020-04-21 2020-12-08 Ирина Амировна Четвертнева Способ получения реагента для обработки буровых растворов
CN111990412B (zh) * 2020-07-21 2021-09-03 广东拉多美化肥有限公司 一种腐植酸复合植物抗高温保护剂及其制备方法
RU2744469C1 (ru) * 2020-09-21 2021-03-09 Федеральное государственное бюджетное образовательное учреждение высшего образования "Самарский государственный медицинский университет" Министерства здравоохранения Российской Федерации Способ получения гуминовых кислот из некондиционных пелоидов
RU2753606C1 (ru) * 2020-10-16 2021-08-18 Николай Иванович Милов Антибактериальное гуминовое средство
RU2756353C1 (ru) * 2020-10-16 2021-09-29 Николай Иванович Милов Иммуномодулирующее гуминовое средство
RU2756364C1 (ru) * 2020-10-16 2021-09-29 Николай Иванович Милов Антикоагуляционное гуминовое средство для улучшения реологических свойств крови
RU2756354C1 (ru) * 2020-10-16 2021-09-29 Николай Иванович Милов Дезинтоксикационное гуминовое средство
RU2753609C1 (ru) * 2020-10-16 2021-08-18 Николай Иванович Милов Противовирусное гуминовое средство
RU2756363C1 (ru) * 2020-10-16 2021-09-29 Николай Иванович Милов Противовоспалительное гуминовое средство
CN112321844A (zh) * 2020-10-29 2021-02-05 云南兴伦肥业有限公司 一种黄腐酸钾的制备工艺
CN113277492B (zh) * 2021-05-20 2022-10-04 新疆心连心能源化工有限公司 一种农林废弃物制备腐植酸钾和生物质炭的方法
CN114702339A (zh) * 2022-02-11 2022-07-05 东华大学 一种利用木质素制备黄腐酸及活性有机肥的方法

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EP0101784A1 (fr) * 1982-08-27 1984-03-07 Egbert Ufheil Procédé pour la préparation d'un formateur d'humus naturel et engrais
US5302180A (en) * 1991-08-28 1994-04-12 Kemiron, Inc. Iron humate product
RU2125039C1 (ru) * 1997-01-14 1999-01-20 Шульгин Александр Иванович Гуминовый концентрат, способ его получения, устройство для электрохимического получения гуминового концентрата (варианты). способ очистки воды от примесей, способ обезвоживания вязкотекучих сред, способ детоксикации органических соединений, способ утилизации осадков сточных вод, способ создания почв из естественных и искусственных грунтов и восстановления плодородия деградированных почв, способ компостирования органических отходов, способ утилизации осадков водопроводных вод

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EP0101784A1 (fr) * 1982-08-27 1984-03-07 Egbert Ufheil Procédé pour la préparation d'un formateur d'humus naturel et engrais
US5302180A (en) * 1991-08-28 1994-04-12 Kemiron, Inc. Iron humate product
RU2125039C1 (ru) * 1997-01-14 1999-01-20 Шульгин Александр Иванович Гуминовый концентрат, способ его получения, устройство для электрохимического получения гуминового концентрата (варианты). способ очистки воды от примесей, способ обезвоживания вязкотекучих сред, способ детоксикации органических соединений, способ утилизации осадков сточных вод, способ создания почв из естественных и искусственных грунтов и восстановления плодородия деградированных почв, способ компостирования органических отходов, способ утилизации осадков водопроводных вод

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115364640A (zh) * 2022-08-03 2022-11-22 广西壮族自治区海洋环境监测中心站 一种改性腐殖酸盐及其在强化氢氧化钙脱硫中的应用
CN115364640B (zh) * 2022-08-03 2023-03-17 广西壮族自治区海洋环境监测中心站 一种改性腐殖酸盐及其在强化氢氧化钙脱硫中的应用

Also Published As

Publication number Publication date
RU2205166C1 (ru) 2003-05-27
UA76563C2 (en) 2006-08-15
EA200400725A1 (ru) 2004-12-30
AU2002362155A1 (en) 2003-06-30
EA006824B1 (ru) 2006-04-28
US20050069974A1 (en) 2005-03-31
US7198805B2 (en) 2007-04-03

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